Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Francesco Tisato' _publ_contact_author_address ; ICIS-CNR Corso Stati Uniti 4 Padova 35127 ITALY ; _publ_contact_author_email TISATO@ICIS.CNR.IT _publ_section_title ; Syntheses and reactivity of 'sulphur rich' Re(III) and Tc(III) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands ; loop_ _publ_author_name 'F. Tisato' 'Giuliano Bandoli' 'Nicolas Lepareur' 'Franck Mevellec' 'Nicolas Noiret' 'Marina Porchia' ; F.Refosco ; data_Re2 _database_code_depnum_ccdc_archive 'CCDC 264127' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 Re S8' _chemical_formula_weight 752.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9840(12) _cell_length_b 12.106(2) _cell_length_c 20.618(4) _cell_angle_alpha 101.61(3) _cell_angle_beta 92.87(3) _cell_angle_gamma 94.22(3) _cell_volume 1455.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 13.7 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 4.759 _exptl_absorpt_correction_type 'psi-scan method' _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet R3m/V four-circle diffractometer' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 5083 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1593 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 26.06 _reflns_number_total 5083 _reflns_number_gt 2702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_cell_refinement 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_data_reduction 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_structure_solution 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_publication_material 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5083 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.33073(9) 0.65016(4) 0.29872(3) 0.04269(18) Uani 1 1 d . . . S1 S 0.5383(5) 0.8257(2) 0.33796(17) 0.0467(9) Uani 1 1 d . . . S2 S 0.0376(5) 0.7214(3) 0.34884(18) 0.0514(9) Uani 1 1 d . . . S3 S 0.1179(5) 0.8887(3) 0.40029(19) 0.0564(10) Uani 1 1 d . . . S4 S 0.1104(5) 0.4795(2) 0.25567(17) 0.0454(9) Uani 1 1 d . . . S5 S 0.5434(5) 0.5587(3) 0.35830(17) 0.0471(9) Uani 1 1 d . . . S6 S 0.4031(6) 0.3903(3) 0.34947(19) 0.0622(11) Uani 1 1 d . . . S7 S 0.2055(6) 0.7062(3) 0.19356(19) 0.0554(10) Uani 1 1 d . . . S8 S 0.6052(5) 0.6092(3) 0.21124(18) 0.0516(9) Uani 1 1 d . . . C1 C 0.3868(17) 0.9220(9) 0.3833(6) 0.039(3) Uani 1 1 d . . . C2 C 0.1919(19) 0.3762(9) 0.2913(6) 0.041(3) Uani 1 1 d . . . C3 C 0.4436(17) 0.6607(9) 0.1579(8) 0.053(4) Uani 1 1 d . . . C1A C 0.488(2) 1.0377(10) 0.4099(6) 0.041(3) Uani 1 1 d . . . C2A C 0.686(2) 1.0752(10) 0.3860(7) 0.051(4) Uani 1 1 d . . . H2AA H 0.7533 1.0276 0.3528 0.061 Uiso 1 1 calc R . . C3A C 0.784(2) 1.1833(11) 0.4114(7) 0.056(4) Uani 1 1 d . . . H3AA H 0.9206 1.2061 0.3964 0.068 Uiso 1 1 calc R . . C4A C 0.684(2) 1.2587(11) 0.4592(7) 0.058(4) Uani 1 1 d . . . C5A C 0.485(2) 1.2225(11) 0.4833(7) 0.056(4) Uani 1 1 d . . . H5AA H 0.4178 1.2710 0.5160 0.067 Uiso 1 1 calc R . . C6A C 0.386(2) 1.1105(10) 0.4579(6) 0.050(3) Uani 1 1 d . . . H6AA H 0.2514 1.0862 0.4736 0.060 Uiso 1 1 calc R . . C7A C 0.797(2) 1.3768(11) 0.4858(7) 0.074(5) Uani 1 1 d . . . C1B C 0.078(2) 0.2582(10) 0.2652(6) 0.047(3) Uani 1 1 d . . . C2B C 0.189(2) 0.1613(10) 0.2705(6) 0.053(4) Uani 1 1 d . . . H2BA H 0.3336 0.1694 0.2906 0.063 Uiso 1 1 calc R . . C3B C 0.087(3) 0.0574(11) 0.2466(7) 0.069(4) Uani 1 1 d . . . H3BA H 0.1611 -0.0056 0.2519 0.083 Uiso 1 1 calc R . . C4B C -0.128(3) 0.0415(12) 0.2136(7) 0.065(4) Uani 1 1 d . . . C5B C -0.235(2) 0.1353(11) 0.2078(8) 0.068(5) Uani 1 1 d . . . H5BA H -0.3780 0.1271 0.1868 0.082 Uiso 1 1 calc R . . C6B C -0.132(2) 0.2410(10) 0.2328(7) 0.061(4) Uani 1 1 d . . . H6BA H -0.2075 0.3036 0.2277 0.074 Uiso 1 1 calc R . . C7B C -0.245(3) -0.0818(11) 0.1859(9) 0.094(6) Uani 1 1 d . . . C1C C 0.488(3) 0.6653(11) 0.0900(7) 0.056(4) Uani 1 1 d . . . C2C C 0.685(2) 0.6188(13) 0.0646(8) 0.072(4) Uani 1 1 d . . . H2CA H 0.7785 0.5841 0.0902 0.086 Uiso 1 1 calc R . . C3C C 0.732(3) 0.6268(15) -0.0001(9) 0.086(6) Uani 1 1 d . . . H3CA H 0.8613 0.5975 -0.0175 0.104 Uiso 1 1 calc R . . C4C C 0.589(4) 0.6786(14) -0.0401(9) 0.082(5) Uani 1 1 d . . . C5C C 0.401(3) 0.7193(15) -0.0125(10) 0.093(6) Uani 1 1 d . . . H5CA H 0.3035 0.7518 -0.0381 0.112 Uiso 1 1 calc R . . C6C C 0.349(3) 0.7149(13) 0.0510(9) 0.085(5) Uani 1 1 d . . . H6CA H 0.2206 0.7453 0.0677 0.102 Uiso 1 1 calc R . . C7C C 0.648(3) 0.6856(16) -0.1112(8) 0.117(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0334(3) 0.0310(3) 0.0608(4) 0.0041(2) -0.0036(2) 0.0033(2) S1 0.0319(19) 0.0318(17) 0.071(3) -0.0013(16) 0.0034(16) -0.0002(14) S2 0.034(2) 0.0377(18) 0.076(3) -0.0016(17) -0.0017(17) 0.0020(15) S3 0.038(2) 0.0398(19) 0.084(3) -0.0051(18) 0.0072(18) 0.0014(15) S4 0.0349(19) 0.0303(17) 0.068(3) 0.0069(16) -0.0075(17) -0.0003(14) S5 0.0375(19) 0.0381(18) 0.063(2) 0.0061(16) -0.0098(16) 0.0031(15) S6 0.068(3) 0.040(2) 0.077(3) 0.0172(19) -0.024(2) 0.0006(18) S7 0.046(2) 0.048(2) 0.076(3) 0.0216(19) -0.0036(19) 0.0093(17) S8 0.040(2) 0.052(2) 0.059(2) 0.0026(18) -0.0026(17) 0.0106(17) C1 0.027(7) 0.030(6) 0.060(9) 0.010(6) -0.003(6) 0.010(5) C2 0.046(8) 0.029(6) 0.048(8) 0.008(6) 0.010(6) 0.000(6) C3 0.011(7) 0.034(7) 0.108(13) 0.006(8) -0.014(7) -0.009(5) C1A 0.037(8) 0.033(7) 0.054(9) 0.011(6) 0.000(6) 0.003(6) C2A 0.047(9) 0.035(7) 0.069(10) 0.005(7) 0.009(7) 0.011(6) C3A 0.040(8) 0.059(9) 0.067(11) 0.011(8) -0.005(7) -0.005(7) C4A 0.068(10) 0.047(9) 0.057(10) 0.010(7) -0.003(8) 0.005(8) C5A 0.069(10) 0.043(8) 0.055(10) 0.006(7) 0.007(8) 0.008(7) C6A 0.053(9) 0.040(8) 0.056(9) 0.003(7) 0.015(7) 0.003(6) C7A 0.084(11) 0.037(8) 0.083(12) -0.014(8) -0.017(9) -0.024(7) C1B 0.058(9) 0.036(7) 0.053(9) 0.016(6) 0.007(7) 0.012(7) C2B 0.057(9) 0.028(7) 0.075(10) 0.015(7) -0.005(7) 0.009(6) C3B 0.084(12) 0.034(8) 0.094(13) 0.021(8) 0.014(10) 0.016(8) C4B 0.065(11) 0.056(10) 0.068(11) -0.002(8) 0.024(8) -0.014(8) C5B 0.055(10) 0.029(7) 0.117(14) 0.013(8) -0.020(9) -0.003(7) C6B 0.043(9) 0.033(7) 0.103(13) 0.005(8) -0.016(8) 0.008(6) C7B 0.121(14) 0.025(8) 0.123(15) 0.000(8) -0.014(11) -0.025(8) C1C 0.072(11) 0.049(9) 0.041(9) 0.001(7) 0.005(8) -0.019(8) C2C 0.055(11) 0.078(11) 0.075(13) -0.001(9) 0.006(9) 0.001(8) C3C 0.078(13) 0.096(13) 0.063(12) -0.031(10) 0.020(10) -0.011(10) C4C 0.098(15) 0.072(12) 0.065(13) 0.000(10) -0.005(12) -0.019(10) C5C 0.108(16) 0.090(14) 0.092(16) 0.037(12) 0.010(13) 0.019(12) C6C 0.108(15) 0.088(13) 0.075(13) 0.039(11) 0.014(11) 0.039(11) C7C 0.19(2) 0.120(16) 0.041(11) 0.021(10) 0.023(12) -0.026(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re S2 2.221(3) . ? Re S5 2.226(3) . ? Re S1 2.352(3) . ? Re S4 2.353(3) . ? Re S7 2.495(4) . ? Re S8 2.501(4) . ? S1 C1 1.690(11) . ? S2 S3 2.098(4) . ? S3 C1 1.701(11) . ? S4 C2 1.662(11) . ? S5 S6 2.116(5) . ? S6 C2 1.674(12) . ? S7 C3 1.713(13) . ? S8 C3 1.672(13) . ? C1 C1A 1.469(14) . ? C2 C1B 1.517(15) . ? C3 C1C 1.449(18) . ? C1A C6A 1.385(15) . ? C1A C2A 1.389(16) . ? C2A C3A 1.382(15) . ? C3A C4A 1.393(17) . ? C4A C5A 1.386(17) . ? C4A C7A 1.519(16) . ? C5A C6A 1.427(15) . ? C1B C6B 1.380(15) . ? C1B C2B 1.409(14) . ? C2B C3B 1.343(16) . ? C3B C4B 1.407(17) . ? C4B C5B 1.367(17) . ? C4B C7B 1.584(17) . ? C5B C6B 1.366(15) . ? C1C C6C 1.376(17) . ? C1C C2C 1.420(18) . ? C2C C3C 1.40(2) . ? C3C C4C 1.42(2) . ? C4C C5C 1.37(2) . ? C4C C7C 1.54(2) . ? C5C C6C 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Re S5 114.91(13) . . ? S2 Re S1 88.80(12) . . ? S5 Re S1 93.83(12) . . ? S2 Re S4 89.95(12) . . ? S5 Re S4 89.38(11) . . ? S1 Re S4 176.79(12) . . ? S2 Re S7 91.26(13) . . ? S5 Re S7 153.27(12) . . ? S1 Re S7 92.01(12) . . ? S4 Re S7 85.06(12) . . ? S2 Re S8 158.51(12) . . ? S5 Re S8 86.51(12) . . ? S1 Re S8 87.93(12) . . ? S4 Re S8 92.16(12) . . ? S7 Re S8 67.65(11) . . ? C1 S1 Re 112.7(4) . . ? S3 S2 Re 111.32(16) . . ? C1 S3 S2 105.3(4) . . ? C2 S4 Re 110.9(4) . . ? S6 S5 Re 110.05(15) . . ? C2 S6 S5 104.1(4) . . ? C3 S7 Re 90.5(5) . . ? C3 S8 Re 91.3(5) . . ? C1A C1 S1 120.1(9) . . ? C1A C1 S3 118.2(9) . . ? S1 C1 S3 121.8(7) . . ? C1B C2 S4 117.5(9) . . ? C1B C2 S6 117.3(8) . . ? S4 C2 S6 125.0(7) . . ? C1C C3 S8 126.6(11) . . ? C1C C3 S7 122.8(10) . . ? S8 C3 S7 110.5(9) . . ? C6A C1A C2A 119.5(11) . . ? C6A C1A C1 120.8(11) . . ? C2A C1A C1 119.7(12) . . ? C3A C2A C1A 120.2(13) . . ? C2A C3A C4A 121.6(13) . . ? C5A C4A C3A 118.9(13) . . ? C5A C4A C7A 121.1(14) . . ? C3A C4A C7A 120.0(14) . . ? C4A C5A C6A 119.7(13) . . ? C1A C6A C5A 120.2(12) . . ? C6B C1B C2B 117.1(12) . . ? C6B C1B C2 121.7(10) . . ? C2B C1B C2 121.1(11) . . ? C3B C2B C1B 120.5(13) . . ? C2B C3B C4B 121.5(12) . . ? C5B C4B C3B 118.1(13) . . ? C5B C4B C7B 121.1(14) . . ? C3B C4B C7B 120.8(13) . . ? C6B C5B C4B 120.3(13) . . ? C5B C6B C1B 122.4(12) . . ? C6C C1C C2C 120.2(15) . . ? C6C C1C C3 122.1(15) . . ? C2C C1C C3 117.7(14) . . ? C3C C2C C1C 117.9(15) . . ? C2C C3C C4C 121.7(16) . . ? C5C C4C C3C 116.8(17) . . ? C5C C4C C7C 123.0(19) . . ? C3C C4C C7C 120.2(19) . . ? C4C C5C C6C 123.5(18) . . ? C5C C6C C1C 119.9(16) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 1.073 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.148 #===END data_Re10 _database_code_depnum_ccdc_archive 'CCDC 264128' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H20 N Re S8' _chemical_formula_weight 705.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 12.503(2) _cell_length_b 10.546(3) _cell_length_c 19.355(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2552.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 12.1 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 5.424 _exptl_absorpt_correction_type 'psi-scan method' _exptl_absorpt_correction_T_min 0.453 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet R3m/V four-circle diffractometer' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 2343 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2343 _reflns_number_gt 2039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_cell_refinement 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_data_reduction 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_structure_solution 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_publication_material 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+8.0400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 2343 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.04612(4) 0.52074(5) 0.7588 0.0382(2) Uani 1 1 d . . . S1 S -0.0597(4) 0.6712(4) 0.6972(3) 0.0467(11) Uani 1 1 d . . . S2 S 0.1116(4) 0.6795(4) 0.8227(3) 0.0493(12) Uani 1 1 d . . . S3 S 0.0201(5) 0.8489(5) 0.8077(3) 0.0560(14) Uani 1 1 d . . . S4 S 0.1470(4) 0.3628(5) 0.8160(3) 0.0508(12) Uani 1 1 d . . . S5 S -0.1039(4) 0.4422(5) 0.8054(3) 0.0464(11) Uani 1 1 d . . . S6 S -0.0671(4) 0.2909(6) 0.8738(3) 0.0577(14) Uani 1 1 d . . . S7 S 0.0207(4) 0.3828(5) 0.6533(3) 0.0551(14) Uani 1 1 d . . . S8 S 0.2005(4) 0.5416(5) 0.6764(3) 0.0471(11) Uani 1 1 d . . . N N 0.1852(15) 0.402(2) 0.5614(13) 0.076(6) Uani 1 1 d . . . C1 C -0.0623(14) 0.8143(17) 0.7386(11) 0.047(6) Uani 1 1 d . . . C2 C 0.0716(17) 0.2693(18) 0.8654(12) 0.050(5) Uani 1 1 d . . . C3 C 0.1389(16) 0.434(2) 0.6207(14) 0.058(6) Uani 1 1 d . . . C1A C -0.1360(17) 0.9115(16) 0.7128(10) 0.045(5) Uani 1 1 d . . . C2A C -0.2325(17) 0.8787(17) 0.6856(12) 0.053(5) Uani 1 1 d . . . H2AA H -0.2488 0.7930 0.6815 0.064 Uiso 1 1 calc R . . C3A C -0.3112(17) 0.971(2) 0.6626(17) 0.060(6) Uani 1 1 d . . . H3AA H -0.3778 0.9474 0.6454 0.072 Uiso 1 1 calc R . . C4A C -0.2789(19) 1.100(2) 0.6685(12) 0.064(6) Uani 1 1 d . . . H4AA H -0.3243 1.1629 0.6522 0.077 Uiso 1 1 calc R . . C5A C -0.185(2) 1.1334(18) 0.6969(14) 0.068(7) Uani 1 1 d . . . H5AA H -0.1698 1.2193 0.7021 0.082 Uiso 1 1 calc R . . C6A C -0.105(3) 1.0418(17) 0.7199(18) 0.081(9) Uani 1 1 d . . . H6AA H -0.0392 1.0660 0.7379 0.097 Uiso 1 1 calc R . . C1B C 0.1108(17) 0.165(2) 0.9072(12) 0.055(5) Uani 1 1 d . . . C2B C 0.073(2) 0.128(3) 0.9718(13) 0.064(6) Uani 1 1 d . . . H2BA H 0.0175 0.1706 0.9938 0.077 Uiso 1 1 calc R . . C3B C 0.126(4) 0.019(4) 1.0032(19) 0.117(16) Uani 1 1 d . . . H3BA H 0.1048 -0.0063 1.0472 0.141 Uiso 1 1 calc R . . C4B C 0.203(3) -0.047(3) 0.973(3) 0.103(13) Uani 1 1 d . . . H4BA H 0.2281 -0.1212 0.9930 0.124 Uiso 1 1 calc R . . C5B C 0.245(6) -0.008(3) 0.913(3) 0.124(15) Uani 1 1 d . . . H5BA H 0.3031 -0.0505 0.8940 0.148 Uiso 1 1 calc R . . C6B C 0.200(3) 0.097(2) 0.8794(15) 0.084(9) Uani 1 1 d . . . H6BA H 0.2285 0.1231 0.8375 0.100 Uiso 1 1 calc R . . C4 C 0.2866(18) 0.454(3) 0.5358(12) 0.065(6) Uani 1 1 d . . . H4A H 0.3367 0.4589 0.5740 0.078 Uiso 1 1 calc R . . H4B H 0.3162 0.3953 0.5020 0.078 Uiso 1 1 calc R . . C5 C 0.277(2) 0.580(4) 0.504(2) 0.106(12) Uani 1 1 d . . . C6 C 0.140(4) 0.282(5) 0.526(3) 0.086(12) Uiso 0.67 1 d P . . C7 C 0.085(5) 0.320(6) 0.463(3) 0.104(17) Uiso 0.67 1 d P . . C6' C 0.099(7) 0.354(7) 0.497(5) 0.066(19) Uiso 0.33 1 d P . . C7' C 0.099(8) 0.218(10) 0.497(6) 0.09(3) Uiso 0.33 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0316(4) 0.0376(4) 0.0453(4) -0.0001(6) -0.0023(5) 0.0000(2) S1 0.047(3) 0.039(2) 0.054(3) -0.008(2) -0.009(2) 0.0004(18) S2 0.057(3) 0.042(2) 0.049(3) -0.001(2) -0.010(3) -0.005(2) S3 0.064(3) 0.045(2) 0.059(3) -0.014(2) -0.017(3) 0.006(2) S4 0.042(3) 0.047(2) 0.064(3) 0.011(2) 0.001(3) 0.0016(19) S5 0.033(2) 0.057(3) 0.049(3) 0.003(2) 0.003(2) 0.0003(19) S6 0.040(3) 0.069(3) 0.064(3) 0.016(3) 0.008(3) -0.001(2) S7 0.038(3) 0.058(3) 0.069(4) -0.026(3) 0.009(3) -0.009(2) S8 0.041(3) 0.049(2) 0.052(3) -0.001(2) 0.000(2) -0.0064(18) N 0.041(10) 0.108(16) 0.079(15) -0.033(13) 0.023(11) -0.013(10) C1 0.039(10) 0.040(9) 0.064(17) -0.009(8) 0.006(9) -0.004(6) C2 0.053(12) 0.038(10) 0.058(13) 0.000(9) 0.000(11) -0.015(8) C3 0.036(10) 0.054(10) 0.084(17) -0.005(11) -0.008(12) 0.002(9) C1A 0.066(13) 0.036(9) 0.032(9) 0.004(7) 0.004(9) -0.012(8) C2A 0.045(11) 0.041(9) 0.073(15) -0.004(9) -0.002(11) 0.015(8) C3A 0.030(10) 0.057(12) 0.09(2) -0.001(12) -0.007(12) 0.007(8) C4A 0.060(15) 0.079(14) 0.052(14) -0.002(11) -0.005(12) 0.026(11) C5A 0.078(16) 0.033(9) 0.093(19) -0.022(10) -0.029(15) 0.004(9) C6A 0.12(2) 0.024(9) 0.10(2) -0.007(11) 0.006(19) -0.005(11) C1B 0.051(13) 0.051(11) 0.061(13) 0.012(10) -0.024(11) -0.012(9) C2B 0.053(14) 0.079(16) 0.061(15) 0.012(12) -0.016(12) -0.008(11) C3B 0.17(4) 0.12(3) 0.07(2) 0.043(19) -0.03(2) -0.08(3) C4B 0.14(4) 0.051(13) 0.12(3) 0.017(18) -0.01(3) 0.011(17) C5B 0.18(4) 0.09(2) 0.10(3) -0.01(2) -0.03(3) 0.07(3) C6B 0.13(3) 0.060(14) 0.062(16) 0.009(12) -0.019(17) 0.021(16) C4 0.044(13) 0.116(18) 0.035(11) -0.006(12) 0.010(10) -0.001(12) C5 0.06(2) 0.14(3) 0.11(3) 0.05(3) -0.01(2) 0.003(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re S2 2.237(5) . ? Re S5 2.240(5) . ? Re S4 2.365(5) . ? Re S1 2.385(5) . ? Re S8 2.513(5) . ? Re S7 2.527(5) . ? S1 C1 1.709(18) . ? S2 S3 2.142(7) . ? S3 C1 1.73(2) . ? S4 C2 1.66(2) . ? S5 S6 2.123(8) . ? S6 C2 1.76(2) . ? S7 C3 1.69(2) . ? S8 C3 1.75(2) . ? N C3 1.33(3) . ? N C4 1.47(3) . ? N C6 1.55(5) . ? N C6' 1.72(9) . ? C1 C1A 1.47(3) . ? C2 C1B 1.45(3) . ? C1A C2A 1.36(3) . ? C1A C6A 1.43(3) . ? C2A C3A 1.45(3) . ? C3A C4A 1.42(3) . ? C4A C5A 1.35(3) . ? C5A C6A 1.46(4) . ? C1B C2B 1.39(3) . ? C1B C6B 1.43(4) . ? C2B C3B 1.47(5) . ? C3B C4B 1.32(6) . ? C4B C5B 1.33(7) . ? C5B C6B 1.41(4) . ? C4 C5 1.47(5) . ? C6 C7' 1.01(10) . ? C6 C6' 1.07(9) . ? C6 C7 1.46(8) . ? C7 C6' 0.78(9) . ? C7 C7' 1.27(11) . ? C6' C7' 1.42(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Re S5 111.1(2) . . ? S2 Re S4 94.18(19) . . ? S5 Re S4 89.85(18) . . ? S2 Re S1 88.96(18) . . ? S5 Re S1 89.00(18) . . ? S4 Re S1 176.87(18) . . ? S2 Re S8 90.25(19) . . ? S5 Re S8 158.56(19) . . ? S4 Re S8 87.11(18) . . ? S1 Re S8 92.90(19) . . ? S2 Re S7 157.48(19) . . ? S5 Re S7 90.40(18) . . ? S4 Re S7 92.3(2) . . ? S1 Re S7 84.80(19) . . ? S8 Re S7 68.54(17) . . ? C1 S1 Re 111.4(7) . . ? S3 S2 Re 110.7(3) . . ? C1 S3 S2 104.3(7) . . ? C2 S4 Re 112.6(8) . . ? S6 S5 Re 110.3(3) . . ? C2 S6 S5 104.7(7) . . ? C3 S7 Re 90.5(8) . . ? C3 S8 Re 89.8(8) . . ? C3 N C4 125(2) . . ? C3 N C6 116(2) . . ? C4 N C6 118(2) . . ? C3 N C6' 115(3) . . ? C4 N C6' 114(3) . . ? C6 N C6' 38(3) . . ? C1A C1 S1 118.1(15) . . ? C1A C1 S3 119.4(14) . . ? S1 C1 S3 122.5(11) . . ? C1B C2 S4 125.3(17) . . ? C1B C2 S6 112.3(15) . . ? S4 C2 S6 122.3(13) . . ? N C3 S7 128.5(18) . . ? N C3 S8 120.4(17) . . ? S7 C3 S8 111.1(14) . . ? C2A C1A C6A 121(2) . . ? C2A C1A C1 120.7(15) . . ? C6A C1A C1 118(2) . . ? C1A C2A C3A 123.3(18) . . ? C4A C3A C2A 115(2) . . ? C5A C4A C3A 122.2(19) . . ? C4A C5A C6A 123.2(19) . . ? C1A C6A C5A 115(3) . . ? C2B C1B C6B 117(2) . . ? C2B C1B C2 127(2) . . ? C6B C1B C2 116(2) . . ? C1B C2B C3B 116(3) . . ? C4B C3B C2B 124(3) . . ? C3B C4B C5B 121(3) . . ? C4B C5B C6B 119(5) . . ? C5B C6B C1B 122(4) . . ? C5 C4 N 114(2) . . ? C7' C6 C6' 86(8) . . ? C7' C6 C7 59(7) . . ? C6' C6 C7 31(5) . . ? C7' C6 N 166(8) . . ? C6' C6 N 80(6) . . ? C7 C6 N 109(4) . . ? C6' C7 C7' 84(10) . . ? C6' C7 C6 45(7) . . ? C7' C7 C6 43(5) . . ? C7 C6' C6 103(10) . . ? C7 C6' C7' 63(8) . . ? C6 C6' C7' 45(6) . . ? C7 C6' N 153(10) . . ? C6 C6' N 62(5) . . ? C7' C6' N 107(7) . . ? C6 C7' C7 79(8) . . ? C6 C7' C6' 49(6) . . ? C7 C7' C6' 33(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.881 _refine_diff_density_min -1.454 _refine_diff_density_rms 0.215 #===END data_Tc10.EtOH _database_code_depnum_ccdc_archive 'CCDC 264129' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 N O S8 Tc' _chemical_formula_weight 662.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.913(2) _cell_length_b 10.414(2) _cell_length_c 14.912(3) _cell_angle_alpha 109.94(3) _cell_angle_beta 90.39(3) _cell_angle_gamma 108.16(3) _cell_volume 1364.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 13.1 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type 'psi-scan method' _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_T_max 0.786 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet R3m/V four-circle diffractometer' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 5044 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5035 _reflns_number_gt 4918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_cell_refinement 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_data_reduction 'P3/P4-PC Vers.4.27 (Nicolet, 1991)' _computing_structure_solution 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _computing_publication_material 'SHELXTL NT Vers.5.10 (Sheldrick, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+3.6532P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5035 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tc Tc 0.14085(4) 0.68817(4) 0.21774(3) 0.04327(14) Uani 1 1 d . . . S1 S 0.06896(14) 0.87158(13) 0.19723(10) 0.0506(3) Uani 1 1 d . . . S2 S -0.05234(14) 0.52357(13) 0.12038(10) 0.0476(3) Uani 1 1 d . . . S3 S -0.16586(15) 0.62245(14) 0.06239(11) 0.0556(3) Uani 1 1 d . . . S4 S 0.21341(14) 0.50941(15) 0.24525(10) 0.0509(3) Uani 1 1 d . . . S5 S 0.33305(15) 0.74350(15) 0.14300(11) 0.0534(3) Uani 1 1 d . . . S6 S 0.45092(14) 0.60588(15) 0.13775(11) 0.0540(3) Uani 1 1 d . . . S7 S 0.28744(17) 0.87544(18) 0.37106(11) 0.0658(4) Uani 1 1 d . . . S8 S 0.00387(15) 0.68869(17) 0.35772(10) 0.0585(3) Uani 1 1 d . . . N N 0.1538(7) 0.8824(7) 0.5273(4) 0.0882(18) Uani 1 1 d . . . C1 C -0.0787(5) 0.8039(5) 0.1179(4) 0.0439(10) Uani 1 1 d . . . C2 C 0.3642(5) 0.4998(5) 0.1997(4) 0.0445(10) Uani 1 1 d . . . C3 C 0.1490(7) 0.8233(7) 0.4324(4) 0.0616(14) Uani 1 1 d . . . C4 C 0.0289(10) 0.8301(12) 0.5764(6) 0.116(3) Uani 1 1 d . . . H4A H -0.0579 0.7913 0.5316 0.140 Uiso 1 1 calc R . . H4B H 0.0215 0.9117 0.6299 0.140 Uiso 1 1 calc R . . C5 C 0.0392(14) 0.7153(15) 0.6134(9) 0.149(5) Uani 1 1 d . . . C6 C 0.2921(10) 0.9889(11) 0.5907(7) 0.110(3) Uani 1 1 d . . . H6A H 0.3059 0.9614 0.6451 0.132 Uiso 1 1 calc R . . H6B H 0.3723 0.9844 0.5542 0.132 Uiso 1 1 calc R . . C7 C 0.2892(19) 1.1285(17) 0.6235(16) 0.244(11) Uani 1 1 d . . . C1A C -0.1389(6) 0.9009(5) 0.0918(4) 0.0479(11) Uani 1 1 d . . . C2A C -0.0558(8) 1.0441(6) 0.1097(5) 0.0736(18) Uani 1 1 d . . . H2AA H 0.0375 1.0794 0.1401 0.088 Uiso 1 1 calc R . . C3A C -0.1102(9) 1.1346(7) 0.0828(6) 0.083(2) Uani 1 1 d . . . H3AA H -0.0534 1.2303 0.0958 0.100 Uiso 1 1 calc R . . C4A C -0.2457(9) 1.0853(8) 0.0378(5) 0.078(2) Uani 1 1 d . . . H4AA H -0.2816 1.1472 0.0205 0.094 Uiso 1 1 calc R . . C5A C -0.3297(8) 0.9435(9) 0.0178(6) 0.084(2) Uani 1 1 d . . . H5AA H -0.4222 0.9093 -0.0137 0.101 Uiso 1 1 calc R . . C6A C -0.2767(7) 0.8512(7) 0.0444(5) 0.0676(16) Uani 1 1 d . . . H6AA H -0.3340 0.7554 0.0305 0.081 Uiso 1 1 calc R . . C1B C 0.4313(5) 0.3987(5) 0.2121(4) 0.0464(11) Uani 1 1 d . . . C2B C 0.3497(7) 0.2752(7) 0.2284(6) 0.0718(18) Uani 1 1 d . . . H2BA H 0.2519 0.2557 0.2304 0.086 Uiso 1 1 calc R . . C3B C 0.4142(8) 0.1808(7) 0.2417(6) 0.084(2) Uani 1 1 d . . . H3BA H 0.3587 0.0990 0.2531 0.100 Uiso 1 1 calc R . . C4B C 0.5575(8) 0.2060(8) 0.2383(6) 0.080(2) Uani 1 1 d . . . H4BA H 0.5989 0.1404 0.2449 0.096 Uiso 1 1 calc R . . C5B C 0.6395(7) 0.3296(8) 0.2250(6) 0.081(2) Uani 1 1 d . . . H5BA H 0.7377 0.3495 0.2248 0.097 Uiso 1 1 calc R . . C6B C 0.5779(6) 0.4245(7) 0.2119(5) 0.0631(15) Uani 1 1 d . . . H6BA H 0.6352 0.5075 0.2027 0.076 Uiso 1 1 calc R . . O O -0.3436(10) 0.5420(14) 0.4865(7) 0.178(4) Uani 1 1 d . . . C1S C -0.413(2) 0.441(3) 0.5189(9) 0.223(10) Uani 1 1 d . . . C2S C -0.536(3) 0.3247(19) 0.5090(11) 0.264(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tc 0.0435(2) 0.0432(2) 0.0513(2) 0.02414(18) 0.00985(17) 0.01746(17) S1 0.0533(7) 0.0377(6) 0.0621(8) 0.0198(6) 0.0000(6) 0.0151(5) S2 0.0503(7) 0.0357(6) 0.0609(7) 0.0206(5) 0.0079(5) 0.0162(5) S3 0.0555(8) 0.0405(6) 0.0685(8) 0.0168(6) -0.0058(6) 0.0167(6) S4 0.0473(7) 0.0544(7) 0.0695(8) 0.0393(6) 0.0191(6) 0.0229(6) S5 0.0531(7) 0.0552(7) 0.0690(8) 0.0398(7) 0.0189(6) 0.0215(6) S6 0.0498(7) 0.0582(8) 0.0702(8) 0.0380(7) 0.0221(6) 0.0228(6) S7 0.0593(8) 0.0679(9) 0.0621(9) 0.0283(7) -0.0006(7) 0.0052(7) S8 0.0504(7) 0.0684(9) 0.0566(8) 0.0224(7) 0.0144(6) 0.0196(6) N 0.098(5) 0.097(4) 0.053(3) 0.019(3) 0.013(3) 0.019(4) C1 0.048(3) 0.040(2) 0.052(3) 0.022(2) 0.014(2) 0.020(2) C2 0.044(2) 0.037(2) 0.053(3) 0.020(2) 0.009(2) 0.0104(19) C3 0.069(4) 0.065(3) 0.055(3) 0.026(3) 0.010(3) 0.023(3) C4 0.108(7) 0.139(8) 0.067(5) 0.006(5) 0.032(5) 0.027(6) C5 0.159(11) 0.175(12) 0.125(9) 0.094(9) 0.045(8) 0.025(9) C6 0.106(7) 0.117(7) 0.081(5) 0.020(5) 0.006(5) 0.019(6) C7 0.195(17) 0.128(12) 0.32(2) -0.040(14) -0.010(16) 0.065(12) C1A 0.055(3) 0.046(3) 0.055(3) 0.024(2) 0.014(2) 0.027(2) C2A 0.080(4) 0.047(3) 0.098(5) 0.028(3) -0.005(4) 0.026(3) C3A 0.103(6) 0.050(3) 0.112(6) 0.037(4) 0.010(5) 0.038(4) C4A 0.106(6) 0.081(5) 0.090(5) 0.053(4) 0.029(4) 0.063(4) C5A 0.073(4) 0.105(6) 0.109(6) 0.061(5) 0.011(4) 0.052(4) C6A 0.060(3) 0.068(4) 0.093(5) 0.046(3) 0.010(3) 0.027(3) C1B 0.043(2) 0.044(3) 0.056(3) 0.021(2) 0.008(2) 0.016(2) C2B 0.051(3) 0.053(3) 0.118(6) 0.042(4) 0.004(3) 0.015(3) C3B 0.073(4) 0.056(4) 0.139(7) 0.053(4) 0.014(4) 0.024(3) C4B 0.078(4) 0.070(4) 0.119(6) 0.051(4) 0.016(4) 0.042(4) C5B 0.058(4) 0.093(5) 0.125(6) 0.065(5) 0.029(4) 0.042(4) C6B 0.051(3) 0.061(3) 0.095(4) 0.045(3) 0.020(3) 0.024(3) O 0.122(7) 0.198(10) 0.147(8) 0.024(7) 0.025(6) 0.007(7) C1S 0.223(18) 0.24(2) 0.081(8) 0.026(10) 0.012(9) -0.054(15) C2S 0.46(4) 0.151(13) 0.125(11) 0.080(11) 0.072(16) -0.015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc S2 2.2208(18) . ? Tc S5 2.2331(15) . ? Tc S1 2.3438(13) . ? Tc S4 2.3459(13) . ? Tc S8 2.4973(16) . ? Tc S7 2.508(2) . ? S1 C1 1.674(5) . ? S2 S3 2.0955(19) . ? S3 C1 1.705(5) . ? S4 C2 1.663(5) . ? S5 S6 2.0962(19) . ? S6 C2 1.711(5) . ? S7 C3 1.705(6) . ? S8 C3 1.712(6) . ? N C3 1.331(8) . ? N C4 1.494(10) . ? N C6 1.524(11) . ? C1 C1A 1.474(6) . ? C2 C1B 1.466(7) . ? C4 C5 1.506(16) . ? C6 C7 1.377(17) . ? C1A C6A 1.389(8) . ? C1A C2A 1.390(8) . ? C2A C3A 1.382(8) . ? C3A C4A 1.357(11) . ? C4A C5A 1.376(10) . ? C5A C6A 1.389(8) . ? C1B C2B 1.391(7) . ? C1B C6B 1.393(7) . ? C2B C3B 1.392(8) . ? C3B C4B 1.367(10) . ? C4B C5B 1.371(9) . ? C5B C6B 1.376(8) . ? O C1S 1.309(19) . ? C1S C2S 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Tc S5 114.02(6) . . ? S2 Tc S1 89.45(5) . . ? S5 Tc S1 91.51(5) . . ? S2 Tc S4 91.96(5) . . ? S5 Tc S4 89.69(5) . . ? S1 Tc S4 177.60(5) . . ? S2 Tc S8 89.22(6) . . ? S5 Tc S8 156.53(6) . . ? S1 Tc S8 91.99(6) . . ? S4 Tc S8 86.09(5) . . ? S2 Tc S7 157.85(6) . . ? S5 Tc S7 87.97(6) . . ? S1 Tc S7 87.21(6) . . ? S4 Tc S7 90.76(6) . . ? S8 Tc S7 69.04(6) . . ? C1 S1 Tc 111.87(17) . . ? S3 S2 Tc 110.64(7) . . ? C1 S3 S2 104.93(18) . . ? C2 S4 Tc 111.90(17) . . ? S6 S5 Tc 110.11(7) . . ? C2 S6 S5 105.19(18) . . ? C3 S7 Tc 89.3(2) . . ? C3 S8 Tc 89.5(2) . . ? C3 N C4 120.5(6) . . ? C3 N C6 121.5(7) . . ? C4 N C6 117.4(6) . . ? C1A C1 S1 120.7(4) . . ? C1A C1 S3 116.5(4) . . ? S1 C1 S3 122.8(3) . . ? C1B C2 S4 120.8(4) . . ? C1B C2 S6 116.2(4) . . ? S4 C2 S6 123.0(3) . . ? N C3 S7 123.4(5) . . ? N C3 S8 124.4(5) . . ? S7 C3 S8 112.2(3) . . ? N C4 C5 113.3(9) . . ? C7 C6 N 111.4(11) . . ? C6A C1A C2A 118.0(5) . . ? C6A C1A C1 121.5(5) . . ? C2A C1A C1 120.4(5) . . ? C3A C2A C1A 120.7(6) . . ? C4A C3A C2A 120.7(7) . . ? C3A C4A C5A 119.8(6) . . ? C4A C5A C6A 120.2(7) . . ? C5A C6A C1A 120.5(6) . . ? C2B C1B C6B 117.5(5) . . ? C2B C1B C2 120.4(5) . . ? C6B C1B C2 122.0(5) . . ? C1B C2B C3B 120.2(6) . . ? C4B C3B C2B 121.2(6) . . ? C3B C4B C5B 119.0(6) . . ? C4B C5B C6B 120.6(6) . . ? C5B C6B C1B 121.4(5) . . ? O C1S C2S 147.5(19) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.918 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.105 #===END